Hydrochloric Acid → 2-[[3-(1,6-dihydro-6-oxo-9H-purin-9-yl)-1-oxopropyl]amino]-3-phenylpropanoic acid

HRID 1534958ノート

反応式

HRID 1534958 の反応式
[O:1]=[C:2]1[NH:10][CH:9]=[N:8][C:7]2[N:6]([CH2:11][CH2:12][C:13]([NH:15][CH:16]([CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[C:17]([O:19]C)=[O:18])=[O:14])[CH:5]=[N:4][C:3]1=2.[OH-].[K+].Cl>O>[O:1]=[C:2]1[NH:10][CH:9]=[N:8][C:7]2[N:6]([CH2:11][CH2:12][C:13]([NH:15][CH:16]([CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[C:17]([OH:19])=[O:18])=[O:14])[CH:5]=[N:4][C:3]1=2

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 1364033592-[[3-(1,6-dihydro-6-oxo-9H-purin-9-yl)-1-oxopropyl]amino]-3-phenylpropanoic acid, methyl ester

生成物 1

HCID 1364033582-[[3-(1,6-dihydro-6-oxo-9H-purin-9-yl)-1-oxopropyl]amino]-3-phenylpropanoic acid収率 83%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

100 mg (0.271 mmol) of 2-[[3-(1,6-dihydro-6-oxo-9H-purin-9-yl)-1-oxopropyl]amino]-3-phenylpropanoic acid, methyl ester (AIT-0085) were placed into a 10 ml beaker equipped with a magnetic stirring bar. Water (5 ml) was added to the beaker and stirring was started. To the stirring heterogeneous mixture was added 100 mg (1.79 mmol) of KOH pellets. Within a few seconds the reaction mixture became a homogeneous green color. Stirring was continued for one hour. The pH of the solution was adjusted to 2.0 with concentrated hydrochloric acid. The product was collected by vacuum filtration and washed twice with 2 ml of water and then twice with 2 ml of acetone. The weight of the product, 2-[[3-(1,6-dihydro-6-oxo-9H-purin-9-yl)1-oxopropyl]amino]-3-phenylpropanoic acid (AIT-0086), was 80 mg. Yield: 83%. m.p. 240°-242° C.

後処理

  1. custombeaker equipped with a magnetic stirring bar
  2. waitWithin a few seconds the reaction mixture became
  3. stirringStirring
  4. filtrationThe product was collected by vacuum filtration
  5. washwashed twice with 2 ml of water

出典と根拠

ORDレコード
ord-8a9b19332cde42b99ef7e70be7320abd
出典データセット
uspto-grants-1992_02
特許番号
US05091432

反応ノート

読み込み中…